CN112675921A - Closed circulation passivation method and passivation system for octenal gas-phase hydrogenation catalyst - Google Patents
Closed circulation passivation method and passivation system for octenal gas-phase hydrogenation catalyst Download PDFInfo
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Abstract
The invention relates to a closed circulation passivation method and a passivation system for an octenal gas-phase hydrogenation catalyst, belonging to the technical field of butanol-octanol gas-phase hydrogenation catalyst passivation. The invention relates to a closed circulation passivation method of an octenal gas phase hydrogenation catalyst, which is characterized in that a circulation loop of a passivation system is replaced by nitrogen, then a hydrogenation reactor is heated, after gas circulation is established for the passivation system, only industrial wind is input to passivate the catalyst, and the passivated tail gas is discharged to a waste gas treatment system. The closed circulation passivation method for the octenal gas phase hydrogenation catalyst, disclosed by the invention, has the advantages of simple process, convenience in operation, improvement of passivation efficiency, great reduction of tail gas emission, reduction of production cost, safety and environmental friendliness; the invention also provides a closed circulation passivation system of the octenal gas phase hydrogenation catalyst, which has scientific and reasonable design.
Description
Technical Field
The invention relates to a closed circulation passivation method and a passivation system for an octenal gas-phase hydrogenation catalyst, belonging to the technical field of butanol-octanol gas-phase hydrogenation catalyst passivation.
Background
The butanol-octanol device of the second fertilizer plant of the petrochemical Qilu division adopts the Dywei/DOW low-pressure rhodium catalyst carbonyl synthesis process to synthesize propylene and synthesis gas (CO, H)2) After toxic impurities are removed by a purification unit as raw materials, butyraldehyde is produced under the catalysis of rhodium-phosphine catalyst, and then butyl alcohol and octanol are prepared through condensation and hydrogenation reactions.
The hydrogenation catalyst is in a reduction state and high in activity when activated, and the reduction-state hydrogenation catalyst can generate spontaneous combustion when meeting air, so that the catalyst needs to be passivated before being discharged, namely the reduction-state catalyst is converted into an oxidation state. The initial deactivation temperature of the catalyst was 150 ℃ and the upper temperature was 270 ℃.
Cu+1/2O2→CuO+37.1kal/mol
The passivation of the butyraldehyde hydrogenation catalyst and the passivation of the octenal hydrogenation catalyst which are originally designed are both passivated by adopting a one-way open method, namely, a hydrogenation reactor is isolated from other equipment and systems, industrial air (purified air) and steam with the pressure of 1.2MPa are introduced from a feeding pipeline at the bottom of the hydrogenation reactor, so that the active component simple substance copper in the hydrogenation catalyst is oxidized with oxygen at the temperature of 150-270 ℃ to generate inert copper oxide, and the passivated generated tail gas is directly discharged into the atmosphere, wherein the adopted device is shown as figure 1.
The original design reinforced catalyst passivation method has the advantages that industrial air and 1.2MPa steam pass through the catalyst bed layer once, so that the consumption is large, the discharged tail gas is large, the passivation efficiency is low, the tail gas is directly discharged into the atmosphere to cause environmental influence and peculiar smell, the method does not meet the current environmental protection requirements and situations, and the method becomes a bottleneck restricting the environmental protection production of the butanol-octanol device.
The exploration of an environment-friendly hydrogenation catalyst passivation method to replace the originally designed one-way open passivation method becomes a breakthrough of the environment-friendly production of the zilubutanol-octanol device, and is necessary to facilitate the upgrading and renovation of the environment-friendly technology of the butanol-octanol industry.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects in the prior art, and providing a closed circulation passivation method for an octenal gas phase hydrogenation catalyst, which has the advantages of simple process, convenient operation, improved passivation efficiency, greatly reduced tail gas emission, reduced production cost, safety and environmental protection; the invention also provides a closed circulation passivation system of the octenal gas phase hydrogenation catalyst, which has scientific and reasonable design.
The invention relates to a closed circulation passivation method of an octenal gas phase hydrogenation catalyst, which is characterized in that a circulation loop of a passivation system is replaced by nitrogen, then a hydrogenation reactor is heated, after gas circulation is established for the passivation system, only industrial wind is input to passivate the catalyst, and the passivated tail gas is discharged to a waste gas treatment system.
The industrial wind is purified air.
The closed circulation passivation method of the octenal gas phase hydrogenation catalyst specifically comprises the following steps:
(a) early preparation: replacing hydrogen and organic matters (octenal and octanol) in the passivation circulation loop by using nitrogen, wherein the volume percentage of the hydrogen in the passivation circulation loop is less than 0.2 percent (v/v), and when the volume percentage of the organic matters is less than 500ppm, the nitrogen is qualified; the nitrogen content in the system after displacement was > 99.5% (v/v).
(b) Heating a hydrogenation reactor: and (3) adding heating steam into the shell pass of the hydrogenation reactor, and heating the bed layer temperature of the hydrogenation reactor to 160-170 ℃.
(c) Establishing gas circulation: adding steam of a heater in front of the hydrogenation reactor, controlling the temperature of gas at the inlet of the hydrogenation reactor to be 150-170 ℃, starting a circulating compressor, and circulating the gas (mostly nitrogen) in the system.
(d) And (3) starting passivation: when purified air is fed, the adding amount is maintained at 330 and 420Kg/h, and the volume percentage content of the oxygen at the inlet of the hydrogenation reactor is maintained at 0.2-0.4%; continuously feeding purified air into the circulation loop, and passivating the octenal hydrogenation catalyst; when the temperature of the catalyst bed layer is respectively raised from 160-170 ℃ to 180-220 ℃ and then falls back to 160-170 ℃ and the oxygen is not consumed in the circulation loop, the passivation of the octenal hydrogenation catalyst is finished; the passivation time is 19 +/-1 h.
(e) And (3) passivating tail gas emission: the passivated tail gas is discharged to a waste gas treatment system RTO for treatment, and the tail gas is converted into H2O、CO2And (4) qualified (meeting relevant national standards) and then discharged after reaching the standard.
In the process, the key process control points are that the temperature of a passivation bed layer is less than 270 ℃, overtemperature is forbidden, and the oxygen content at the inlet of a hydrogenation reactor is controlled to be 0.2-0.4% (v/v).
In the closed circulation passivation system for the octenal gas-phase hydrogenation catalyst, an evaporator is sequentially connected with a heater, a hydrogenation reactor, a cooler, a collecting tank and a circulation compressor to form a circulation loop; the industrial air inlet pipeline is connected with the evaporator; the line connecting the cooler to the collecting tank is connected to an exhaust gas treatment system.
The invention utilizes the original collecting tank, the circulating compressor, the evaporator, part of pipelines and the hydrogenation reactor to form a circulating loop; the bottom feeding pipeline of the hydrogenation reactor is only filled with industrial air (purified air), the circulating compressor is utilized to lead the passivation gas to flow away and be recycled in the circulating loop, the industrial air consumption is reduced, a small amount of tail gas generated at the same time is discharged to the waste gas treatment device RTO (regenerative thermal oxidizer) for treatment, the tail gas is discharged after reaching the standard, and the environmental protection problem is thoroughly eliminated.
The closed circulation passivation method only adopts the circulating gas (nitrogen) as a carrier of purified air (the effective component is oxygen) required by passivation, provides the functions of diluting and dispersing the purified air, takes away heat generated in the passivation process by the circulating gas, and circularly cools in a hydrogenation outlet cooler to keep heat balance; the method reduces the heat generated by diluting, dispersing and purifying air and carrying away passivation by using 1.2MPa steam as passivation in the traditional passivation, reduces the consumption of 1.2MPa steam by 3t/h, which is 126t in total, reduces the passivation time from 42h to 19 +/-1 h, and reduces the emission of the tail gas of 110-.
The invention explores a new method which is more environment-friendly and efficient and is suitable for the passivation of the hydrogenation catalyst in the butanol and octanol industry, replaces the originally designed catalyst passivation method, and carries out technical upgrading and innovation on the passivation method of the hydrogenation catalyst in the butanol and octanol industry; the problems of peculiar smell, tail gas emission and the like generated in the passivation process of the hydrogenation catalyst of the butanol-octanol device are solved; the method is suitable for new and stricter environmental protection situations and trends, eliminates the environmental protection bottleneck of the passivation process of the gas-phase hydrogenation catalyst in the existing butanol and octanol industry, and promotes the environmental protection of the butanol and octanol industry.
Compared with the prior art, the invention has the following beneficial effects:
(1) the closed circulation passivation method for the octenal gas phase hydrogenation catalyst has the advantages of simple process, convenient operation, improvement of passivation efficiency, reduction of passivation time from 42h to 19 +/-1 h, great reduction of tail gas emission, emission reduction of 110 t and 120t of tail gas, reduction of production cost, safety and environmental protection;
(2) the closed circulating passivation system for the octenal gas-phase hydrogenation catalyst is scientific and reasonable in design and simple and convenient to operate;
(3) according to the invention, through the technical problems of overcoming and solving, the gas-phase hydrogenation catalyst closed cycle passivation in the butanol-octanol industry is realized for the first time, the method is efficient and environment-friendly, one hand of experience of a new gas-phase hydrogenation catalyst passivation method in the davidi octanol process is summarized, and one hand of information of the application condition of the closed cycle passivation in the davidi process butanol-octanol device is mastered;
(4) the gas-phase hydrogenation catalyst in the butanol-octanol industry is passivated in a closed cycle manner, so that the environmental protection problems that the tail gas of the gas-phase hydrogenation catalyst passivated by the zilu butanol-octanol device is directly discharged into the atmosphere and the surrounding peculiar smell is serious are successfully solved, the passivation efficiency is improved by breaking through the passivation environment protection bottleneck of the gas-phase hydrogenation catalyst, and considerable environmental protection, economic and technical benefits are created.
Drawings
FIG. 1 is a schematic diagram of the apparatus used in the prior art for the passivation of octenal vapor phase hydrogenation catalysts;
FIG. 2 is a schematic view of a closed cycle passivation system for an octenal vapor phase hydrogenation catalyst according to the present invention;
in the figure: 1. a 1.2MPa steam admission line; 2. a hydrogenation reactor; 3. an exhaust gas discharge line; 4. a cooler; 5. collecting tank; 6. a recycle compressor; 7. a gate valve; 8. an evaporator; 9. a heater; 10. an industrial wind inlet pipeline; 11. an exhaust gas treatment system.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
As shown in fig. 2, in the closed circulation passivation system for the octenal gas-phase hydrogenation catalyst, an evaporator 8 is sequentially connected with a heater 9, a hydrogenation reactor 2, a cooler 4, a collecting tank 5 and a circulation compressor 6 to form a circulation loop; the industrial wind inlet pipeline 10 is connected with the evaporator 8; the line connecting cooler 4 to collecting tank 5 is connected to an exhaust gas treatment system 11.
Example 1
The closed circulation passivation method of the octenal gas phase hydrogenation catalyst specifically comprises the following steps:
(1) early preparation: replacing hydrogen (the volume percentage content is 72% (v/v)), organic matters (the octenal content is 0.1% (v/v) and the octanol content is 3.9% (v/v)) in the passivation circulation loop with nitrogen to be qualified; after the nitrogen is replaced qualified, the volume percentage of hydrogen in the passivation circulation loop is less than 0.2 percent, the volume percentage of organic matters is less than 500ppm, and the volume percentage of nitrogen is 99.5 (v/v).
(2) Heating a hydrogenation reactor: and (3) feeding heating steam to the shell side of the hydrogenation reactor 2, and heating the bed layer temperature of the hydrogenation reactor 2 to 165 ℃.
(3) Establishing gas circulation: adding steam of a heater in front of the hydrogenation reactor 2, controlling the temperature of gas at the inlet of the hydrogenation reactor 2 at 160 ℃, starting a circulating compressor 6, and circulating the gas (mostly nitrogen) in the system.
(4) And (3) starting passivation: when purified air is fed, the feeding amount is maintained at 370Kg/h, and the volume percentage of oxygen at the inlet of the hydrogenation reactor 2 is maintained at 0.4%. Continuously feeding purified air into the circulation loop, and passivating the octenal hydrogenation catalyst; when the temperature of the catalyst bed layer is respectively increased from 165 ℃ to 190 ℃ (peak value), the temperature falls back to 165 ℃, oxygen is not consumed in a circulation loop any more, and the passivation of the octenal hydrogenation catalyst is finished; the passivation time was 19 h.
(5) And (3) passivating tail gas emission: the passivated tail gas is discharged to a waste gas treatment system RTO 11 for treatment, and the tail gas is converted into H2O、CO2And (5) discharging after the product is qualified.
Compared with the prior art, the process in the embodiment reduces the emission of the tail gas by about 120t, and reduces the passivation time by 22.7 h.
Example 2
The closed circulation passivation method of the octenal gas phase hydrogenation catalyst specifically comprises the following steps:
(1) early preparation: replacing hydrogen (with the volume percentage content of 70% (v/v)), organic matters (with the content of 0.1% (v/v) for octenal and 3.9% (v/v) for octanol) in the passivation circulation loop by using nitrogen to be qualified; after the nitrogen is replaced qualified, the volume percentage of hydrogen in the passivation circulation loop is less than 0.2 percent, the volume percentage of organic matters is less than 500ppm, and the volume percentage of nitrogen is 99.5 (v/v).
(2) Heating a hydrogenation reactor: and (3) feeding heating steam to the shell pass of the hydrogenation reactor 2, and heating the bed layer temperature of the hydrogenation reactor 2 to 160 ℃.
(3) Establishing gas circulation: adding steam of a heater 9 in front of the hydrogenation reactor 2, controlling the temperature of gas at the inlet of the hydrogenation reactor 2 at 150 ℃, starting a circulating compressor 6, and circulating the gas (mostly nitrogen) in the system.
(4) And (3) starting passivation: when purified air is fed, the feeding amount is maintained at 330Kg/h, and the volume percentage of oxygen at the inlet of the hydrogenation reactor 2 is maintained at 0.2%. Continuously feeding purified air into the circulation loop, and passivating the octenal hydrogenation catalyst; when the temperature of the catalyst bed layer is respectively increased from 160 ℃ to 180 ℃ (peak value), the temperature falls back to 160 ℃, and the oxygen is not consumed in the circulation loop any more, and the passivation of the octenal hydrogenation catalyst is finished; the passivation time was 18 h.
(5) And (3) passivating tail gas emission: the passivated tail gas is discharged to a waste gas treatment system RTO 11 for treatment, and the tail gas is converted into H2O、CO2And (5) discharging after the product is qualified.
Compared with the prior art, the process in the embodiment reduces the emission of the tail gas by about 118t, and the passivation time is reduced by 23.9 h.
Example 3
The closed circulation passivation method of the octenal gas phase hydrogenation catalyst specifically comprises the following steps:
(1) early preparation: replacing hydrogen (with the volume percentage content of 76% (v/v)), organic matters (with the content of octenal of 0.1% (v/v) and octanol of 3.9% (v/v)) in the passivation circulation loop by using nitrogen to be qualified; after the nitrogen is replaced qualified, the volume percentage of hydrogen in the passivation circulation loop is less than 0.2 percent, the volume percentage of organic matters is less than 500ppm, and the volume percentage of nitrogen is 99.5 (v/v).
(2) Heating a hydrogenation reactor: and (3) adding heating steam into the shell pass of the hydrogenation reactor 2, and heating the bed layer temperature of the hydrogenation reactor 2 to 170 ℃.
(3) Establishing gas circulation: adding steam of a heater 9 in front of the hydrogenation reactor 2, controlling the temperature of gas at the inlet of the hydrogenation reactor 2 at 170 ℃, starting a circulating compressor 6, and circulating the gas (mostly nitrogen) in the system.
(4) And (3) starting passivation: when purified air is fed, the adding amount is maintained at 420Kg/h, and the volume percentage of oxygen at the inlet of the hydrogenation reactor 2 is maintained at 0.3%. Continuously feeding purified air into the circulation loop, and passivating the octenal hydrogenation catalyst; when the temperature of the catalyst bed layer is respectively increased from 170 ℃ to 220 ℃ (peak value), the temperature falls back to 170 ℃, oxygen is not consumed in a circulation loop any more, and the passivation of the octenal hydrogenation catalyst is finished; the passivation time was 20 h.
(5) And (3) passivating tail gas emission: the passivated tail gas is discharged to a waste gas treatment system RTO 11 for treatment, and the tail gas is converted into H2O、CO2And (5) discharging after the product is qualified.
Compared with the prior art, the process in the embodiment reduces the emission of the tail gas by about 115t, and the passivation time is reduced by 22.1 h.
The process of the invention is successfully applied to the second fertilizer plant of the Qilu division company for the first time, is the first time in the industry of butanol and octanol, is a creative innovation of the passivation process of the hydrogenation catalyst in the industry of butanol and octanol, and can be popularized and applied in the industry.
As shown in fig. 1, in the prior art, a single-pass open method is adopted for passivation, a hydrogenation reactor 2 is isolated from other equipment and systems (a gate valve 7 is arranged on a pipeline connecting an evaporator and the hydrogenation reactor 2, and a gate valve 7 is also arranged on a pipeline connecting the hydrogenation reactor 2 and a cooler 4), industrial air (purified air) and 1.2MPa steam are introduced from a feeding pipeline at the bottom of the hydrogenation reactor 2, so that an active component elemental copper in a hydrogenation catalyst is subjected to oxidation reaction with oxygen at 150-270 ℃ to generate inert copper oxide, and the passivated generated tail gas is directly discharged to the atmosphere.
Comparative example 1
Adopts the one-way open passivation process of the prior art to passivate the octenal hydrogenation catalyst, and comprises the following steps:
(1) early preparation: the hydrogenation reactor 2 is isolated by a blind plate (as shown in figure 1), and the hydrogen (72 percent by volume (v/v)), the organic matter (0.1 percent by volume (v/v) of octenal and 3.9 percent by volume (v/v)) in the hydrogenation reactor 2 are replaced by nitrogen to be qualified; after the nitrogen replacement is qualified, the volume percentage of the hydrogen in the hydrogenation reactor 2 is less than 0.2 percent, the volume percentage of the organic matter is less than 500ppm, and the volume percentage of the nitrogen is 99.5 (v/v).
(2) Heating a hydrogenation reactor: 1.2MPa steam is fed from the inlet of the hydrogenation reactor 2, the feeding amount is maintained at 3.8t/h, high-temperature steam passes through the catalyst bed layer from bottom to top, the high-temperature steam is discharged from the top of the hydrogenation reactor 2, the temperature of the bed layer of the hydrogenation reactor 2 is raised to 165 ℃, and tail gas is generated at the same time at 3.8 t/h.
(3) And (3) starting passivation: feeding purified air from the inlet of the hydrogenation reactor 2, keeping the amount of the purified air at 200Kg/h, controlling the volume percentage of oxygen in the hydrogenation reactor 2 to be 3.2% (v/v), and passivating the octenal hydrogenation catalyst; when the temperature of the catalyst bed layer is respectively increased from 165 ℃ to the peak temperature (200 ℃ is higher than the peak temperature and is lower than 270 ℃), the temperature falls back to 165 ℃, and the hydrogenation reactor does not consume oxygen any more, the passivation of the octenal hydrogenation catalyst is finished; the passivation time was about 42 h.
(4) And (3) passivating tail gas emission: the volume content of organic matters in the discharged tail gas is 200ppm-500ppm, and the discharge amount is 126 t.
Claims (10)
1. A closed circulation passivation method for an octenal gas phase hydrogenation catalyst is characterized by comprising the following steps: and (3) replacing a circulation loop of the passivation system by using nitrogen, then heating the hydrogenation reactor (2), after establishing gas circulation on the passivation system, only inputting industrial wind to passivate the catalyst, and discharging the passivated tail gas to a waste gas treatment system (11).
2. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 1, characterized in that: the industrial wind is purified air.
3. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 2, characterized in that: the method specifically comprises the following steps:
(a) early preparation: replacing hydrogen and organic matters in the passivation circulation loop with nitrogen to be qualified;
(b) heating a hydrogenation reactor: heating steam is fed into the shell pass of the hydrogenation reactor (2), and the bed temperature of the hydrogenation reactor (2) is raised to 160-170 ℃;
(c) establishing gas circulation: adding steam of a heater (9) in front of the hydrogenation reactor (2), controlling the temperature of gas at the inlet of the hydrogenation reactor (2) to be 150-170 ℃, starting a circulating compressor (6), and circulating the gas in the system;
(d) and (3) starting passivation: continuously feeding purified air into the circulation loop, and passivating the octenal hydrogenation catalyst;
(e) and (3) passivating tail gas emission: and the passivated tail gas is discharged to a waste gas treatment system (11) for treatment.
4. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 3, characterized in that: the qualified standard for nitrogen replacement in the step (1) is as follows: the volume percentage of hydrogen in the passivation circulation loop is less than 0.2 percent, and the volume percentage of organic matters is less than 500 ppm.
5. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 3, characterized in that: the volume content of nitrogen in the system after the replacement in the step (1) is more than 99.5 percent.
6. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 3, characterized in that: when purified air is started to be fed, the feeding amount is maintained at 330 and 420Kg/h, and the volume percentage of oxygen at the inlet of the hydrogenation reactor (2) is maintained at 0.2-0.4%.
7. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 3, characterized in that: in the step (4), when the temperature of the catalyst bed is respectively raised from 160-170 ℃ to 180-220 ℃ and then falls back to 160-170 ℃, and the oxygen is not consumed in the circulation loop, the passivation of the octenal hydrogenation catalyst is finished.
8. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 3, characterized in that: in the step (4), the passivation time is 19 +/-1 h.
9. The closed cycle passivation method of octenal gas phase hydrogenation catalyst according to claim 3, characterized in that: in the step (5), the tail gas is converted into H2O、CO2And (5) discharging after the product is qualified.
10. A closed cycle deactivation system for octenal vapor phase hydrogenation catalyst according to any one of claims 1 to 9, characterized in that: the evaporator (8) is sequentially connected with the heater (9), the hydrogenation reactor (2), the cooler (4), the collecting tank (5) and the circulating compressor (6) to form a circulating loop; the industrial air inlet pipeline (10) is connected with the evaporator (8); the line connecting the cooler (4) and the collecting tank (5) is connected to an exhaust gas treatment system (11).
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